We developed an integrated analytical procedure for organochlorine contaminants that enables quantitation of toxaphene residues as low as 0.1 gg/g in fish tissue. Preparation of the sample requires extraction of ground tissue with dichloromethane, cleanup of the extract by gel permeation chromatography, and fractionation by Florisil and silica gel chromatography. Toxaphene residues are then characterized and quantified by capillary-column gas chromatography with electron capture. An automated data system is used to select and quantitate peaks and to eliminate interference from the high-resolution chromatograms. Selected components are then confirmed by gas chromatography-negative-ion mass spectrometry (NIMS).This procedure consistently yields results within 1% of spike concentrations. Substitution of conventional packed-column gas chromatography into the procedure reduces accuracy slightly; values average 7% below spiked concentrations. We also evaluated several confirmation techniques and other methods for eliminating analytical interferences. Nitration of the toxaphene-containing fraction before gas chromatography successfully eliminated interferences from the DDT complex but not from chlordane components. This procedure also altered the composition of the toxaphene mixture. Among the gas chromatography-mass spectrometry confirmation procedures evaluated, NIMS proved superior to the more conventional electron-impact mass spectrometry because toxaphene components were far more sensitive to NIMS.